期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1642, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.chroma.2021.462039
关键词
Steroids; Sulfates; Gas Chromatography; Open Screening; Doping; High Resolution
资金
- Partnership for Clean Competition [2019R2000409G]
The World Anti-Doping Agency (WADA) sets strict requirements for anti doping laboratories to comply with, including using gas chromatography - mass spectrometry (GC-MS) and liquid chromatography MS (LC-MS) for initial testing procedure (ITP) to improve detection time. However, a LC-MS ITP combining sulfated AAS with other mandatory targets has not been developed yet, which is crucial for economical purposes.
The World Anti-Doping Agency (WADA) publishes yearly their prohibited list, and sets a minimum required performance limit for each substance. To comply with these stringent requirements, the anti doping laboratories have at least two complementary methods for their initial testing procedure (ITP), one using gas chromatography - mass spectrometry (GC-MS) and the other using liquid chromatography MS (LC-MS). Anabolic androgenic steroids (AAS) have in previous years consistently been listed as the most frequently detected class of compounds. Over the last decade, evidence has emerged where a longer detection time is attained by focusing on sulfated metabolites of AAS instead of the conventional gluco-conjugated metabolites. Despite a decade of research on sulphated AAS using LC-MS, no LC-MS ITP has been developed that combines this class of compounds with the other mandatory targets. Such combination is essential for economical purposes. Recently, it was demonstrated that the direct injection of non-hydrolysed sulfates is compatible with GC-MS. Using this approach and by taking full use of the open screening capabilities of the quadrupole time of flight MS (QTOF-MS), this work describes for the first time a validated ITP that allows the detection of non-hydrolysed sulfated metabolites of AAS while, simultaneously, remaining capable of detecting a vast range of other classes of compounds, as well as the quantification of endogenous steroids, as required for an ITP compliant with the applicable WADA regulations. The method contains 263 compounds from 9 categories, including stimulants, narcotics, anabolic androgenic steroids and beta-blockers. Additionally, the advantages of the new method were illustrated by analysing excretion samples of drostanolone, mesterolone and metenolone. No negative effects were observed for the conventional markers and the detection time for mesterolone and metenolone increased by up to 150% and 144%, respectively compared to conventional markers.
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